Transmission electron microscopy investigation of pulsed-laser deposited hydroxylapatite thin films prepared by tripod and focused ion beam techniques

被引:13
作者
Iliescu, M
Nelea, V
Werckmann, J
Mihailescu, IN
机构
[1] Inst Phys & Chim Mat, Grp Surfaces Interfaces, F-67037 Strasbourg, France
[2] Inst Natl Sci Appl, Lab Ingn Surfaces, F-67084 Strasbourg, France
[3] Natl Inst Lasers Plasma & Radiat Phys, Lasers Dept, Bucharest 77125, Romania
关键词
biocompatible and bioactive thin films; hydroxylapatite thin films; pulsed laser deposition; electron microscopy; focused ion beam; mechanical polishing with tripod;
D O I
10.1016/j.surfcoat.2004.01.022
中图分类号
TB3 [工程材料学];
学科分类号
0805 ; 080502 ;
摘要
Hydroxylapatite-based ceramics are largely applied as coatings and thin films on metallic components of prostheses for inducing osteoblasts apposition and subsequent bone re-growth. We report for the first time the focused ion beam technique (FIB) as a milling method to prepare specimens for transmission electron microscopy investigations of HA thin films gown on metallic substrates. New FIB technique results were compared to those obtained by the thinning method of mechanical polishing with tripod. HA films were obtained by pulsed laser deposition on Si wafers and polished Ti-5Al-2.5Fe substrates coated with TiN buffer layers. A KrF* excimer laser (lambda = 248 nm, tau(FWHM) greater than or equal to20) was used for deposition. HA films were grown in vacuum (10(-4) Pa) on room temperature substrates, subsequently annealed at 550 degreesC in ambient air for 1 h. Processed structures were investigated by transmission electron microscopy (TEM), grazing incidence X-ray diffraction, selected area electron diffraction, and energy dispersive X-ray spectroscopy. We show that both tripod polishing and focused ion beam milling techniques well preserve the structural and chemical integrity of the thin layers, and their interfaces. Additionally, focused ion beam milling allows for preparation of long specimens (approx. 12 mum in our case). HA films were stoichiometric and had a nano-crystalline structure with an average grain size of 35 mum. Cross-section TEM patterns show a granular growth morphology of the films. Particulates trapped within the film were visualized. High resolution TEM analysis shows that the transition from cubic TiN to hexagonal HA is intermediated by a very thin amorphous calcium phosphate interlayer of similar to 3 -4 nm thickness. (C) 2004 Published by Elsevier B.V.
引用
收藏
页码:131 / 140
页数:10
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